Effective, controlled turbulent mixing for flow chemistry

18 Jan 2021
Tom Casburn
Associate Editor

The Uniqsis range of Glass Static Mixer (GSM) chip reactor blocks produce an efficient, turbulent mixed reagent stream for flow chemistry reactions that is not diffusion dependent.

To achieve highly reproducible flow chemistry scale-up the control of mixing and temperature is essential, particularly for highly exothermic or fast, mixing-dependent reactions.

Now available in sizes from 270µl to 20 ml, the recently expanded range of GSM chips from Uniqsis can be used to perform reactions from -80°C to over 150°C. GSM chips up to 2 ml can be operated up to 40-bar and are available in 2-channel or 3-channel inlet configurations. Larger GSM chips of 10ml and 20 ml have a premixing channel followed by a residence domain and can operate up to 10-bar.

GSM chips can be used as mixing modules prior to a coil reactor residence time unit, or as reactor blocks for rapid exothermic reactions such as nitrations. Nitration is an important synthetic procedure that, following reduction of the nitro group, provides a useful route for the introduction of amino groups onto aromatic rings. Uniqsis Application Note 22 describes how a GSM chip was used to control both temperature and mixing. Under these controlled conditions, selective mono-nitration was rapidly performed at elevated temperature to maximize throughput.

Uniqsis GSM chips are precision machined from inert borosilicate glass to withstand a wide temperature range and can be conveniently attached to a FlowSyn column heater module, Cold Coil, or Polar Bear Plus cryogenic reactor modules.

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FlowSyn Continuous Flow Reactor

Uniqsis Ltd

FlowSyn - Making Flow Chemistry Simple FlowSyn is a fully integrated continuous flow reactor with everything you need to start doing flow chemistry including reaction optimization, synthesis and scale up. To provide maximum flexibility, a wide range of mixer and reactor options are available as well as additional modules for performing multiple experiments, or sub-ambient chemistry. • Ability to perform continuous flow chemistry under microwave-like conditions (up to 260oC). • Perform sub-ambient continuous flow chemistry using the 'Cold Coil'. • Run up to 10 automated sequential experiments with the 'Automated Experiment Package'.A pair of high pressure pumps are used to deliver reagent solutions from either stock bottles or sample injection loops through a 'T'-mixer into the electrically heated flow reactors. Reactions can be heated to 260?C and 150?C in the coil and column reactor modules respectively. Back pressure regulators of up to 1000 psi are used to pressurise the system and thus perform superheating of solvents, allowing the chemist to access'microwave like' conditions with no limitation on scale. FlowSyn is very easy to use with a high resolution user interface. The user is guided through the process for setting up a flow chemistry reaction by inputting parameters for reagent volumes, temperatures and reaction times. The user can choose to collect all of the reaction plug, or only the 'steady state' part. FlowSyn will then equilibrate and run the reaction, and finally flush the system through with solvent. Throughout FlowSyn will monitor the pressure of the system, and shut down if a problem occurs allowing FlowSyn to be safely run unattended.

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